HRID1267734

反应详情

EQUATION

反应方程式

HRID 1267734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium iodide (35.1 g, 2.15 mol) was added to a solution of 1-methanesulfonyloxy-4,4,5,5,5-pentafluoropentane (20 g, 0.781 mol) in acetone (200 ml), followed by heating under reflux for 12 hours. After the reaction mixture was filtered, the filtrate was concentrated. Ethyl acetate was added to the residue, which was then filtered again. The filtrate was washed with water and saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate. The solvent was distilled off to give 1-iodo-4,4,5,5,5-pentafluoropentane (21.1 g, Yield 93.4%).

WORKUP

后处理

  1. temperatureby heating
  2. temperatureunder reflux for 12 hours
  3. filtrationAfter the reaction mixture was filtered
  4. concentrationthe filtrate was concentrated
  5. additionEthyl acetate was added to the residue, which
  6. filtrationwas then filtered again
  7. washThe filtrate was washed with water and saturated aqueous sodium chloride
  8. dry with materialdried over anhydrous magnesium sulfate
  9. distillationThe solvent was distilled off